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Harmaline/harmine to THH - safe kitchen conversion tek required. Again.

Migrated topic.
eventually may be today ...

harmine disolved in ethanol + hydrochloric acid
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under uv
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zink added and 5 minutes passed
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uv
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starting product on the left - harmine
end product as freebase on the right -

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The freebase is far too heavy so separation is required - thh precips at around pH 6.9 - could that be the method of separation ?
 
what else - besides ammonium chloride can be added to prevent the zink from precipping ?
 
ethyl acetate is found in acetone free nail polish remover and can be distilled off easily.

ammonium chloride: just neutralize some HCl with ammonia and evaporate

harmine precips at PH = 8.75 or above, while harmaline precips at the higher PHs:

Harmine becomes a freebase in a pH where most harmaline is still salt, so one can separate them. If you have accurate pH meter, at pH 8,75, 92% of harmine will precipitate while only 8% of harmaline will precipitate.
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(wiki)

If THH really precips at 6.9 we are in good shape :D
 
dagger, I found elemental zinc easily in walk-in chemical supply stores in a major city of southern europe. Dont you have these kind of stores, chemical/lab supply stores, in the nearest city to you? These kind of stores have catalogues of main chemical suppliers so they can order things for you even if its not in stock.
 
endlessness said:
dagger, I found elemental zinc easily in walk-in chemical supply stores in a major city of southern europe. Dont you have these kind of stores, chemical/lab supply stores, in the nearest city to you? These kind of stores have catalogues of main chemical suppliers so they can order things for you even if its not in stock.
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Not much around here were I live. I see that you can buy 99% zinc powder on ebay. Would this be good enough, or could there be some undesirable impurities in it?
 
instead basifying with ammonia in the end, can one use sodium carbonate or lye instead? I don't get the chemistry behind this at all.
 
Ok, so I was wondering. If the reaction causes excess unwanted salts, is it possible to get rid of these salts by performing a manske on the final product where the THH precips as Hcl's and the unwanted salts stay in solution? I'm probably going to try this out sometime in the next week, unless anyone has a good reason why this won't work?

Well here's what's happened so far.

I weighed out 500mg of harmaline that was slightly pinky/white and added it to a solution of 100ml hcl 10% then stirred thoroughly until a clear amber solution was formed.

I then added enough zinc to leave a fairly thick (about 5mm) covering on the bottom of the glass. This was then sat in a tub of hot water and stirred until a bubbling reaction occurred. Over the next 30 minutes the colour of the solution became a lot more pale until the solution was more or less clear with maybe the slightest tint of yellow.

It's still bubbling away, so I shall leave it until the bubbling stops then filter the zinc out of the solution.

After that I'm going to dilute the solution with an equal amount of water, bring to a boil and salt saturate to hopefully precipitate THH Hcl. The final product shall be weighed.

Well the solution has been salted now and it's cooled a little and gotten very cloudy. However I'm noticing some squre crytal formations, so I'm guessing that this is salt? I've never seen a THH crystal, but I'd imagine that it wouldn't be square. Anyways whatever comes out overnight I shall redesolve and then freebase.

Yep. Definately lots of salt as it was waaay heavy. Anyway I've now redesolved the salt/stuff in acidic water and based the stuff and now I have some very fluffy white precips coming out. I'll give it a few hours then filter, dry and weigh. Hopefully I'll have the right result.
 
Dagger said:
I'd love to try this method, but here in europe I have a hard time finding elemental zinc. Is there anything else that can be tried? Aluminium, iron or anything else?
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Same here. I know that zinc amalgam could perhaps be used. Powdered zinc is also available in some places. Do let me know what happens with this, as I'd like to claim ALL THE CREDIT since I found ONE PAPER and posted it up ;) hehe
 
Right I know there has been a lot of yes and no's on the subject, but I don't think THH precips in a manske. I redesolved what was indeed mostly rock salt and basified and only a few scraps of what is probably unreacted harmaline dropped out. I'm guessing less than 80mg. But it's a good sign that if it was harmaline there would have been a lot more precips, so whatever it has become, it isn't harmaline anymore.

I'm pretty glad I didn't throw away the salty water now and have based that and now there are a shitload of what I'm hoping is THH and reaction byproduct which I shall filter out, redesolve and base to pH 7 which hopefully will only precip THH.

I'm telling you though... the process from seeds to this stage has been a long one. I'll probably cry if this hasn't worked :)
 
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